CN110437202A - A kind of chloridization process of ethylene carbonate - Google Patents
A kind of chloridization process of ethylene carbonate Download PDFInfo
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- CN110437202A CN110437202A CN201910796829.XA CN201910796829A CN110437202A CN 110437202 A CN110437202 A CN 110437202A CN 201910796829 A CN201910796829 A CN 201910796829A CN 110437202 A CN110437202 A CN 110437202A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D317/00—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms
- C07D317/08—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3
- C07D317/10—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings
- C07D317/32—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D317/42—Halogen atoms or nitro radicals
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Abstract
The invention discloses a kind of chloridization process of ethylene carbonate, comprising the following steps: liquid chlorine vaporizing S1, is obtained chlorine, is then fed into the mixing section of chlorination reactor；S2, ethylene carbonate is preheated at 36~40 DEG C, obtains melting ethylene carbonate, and be added in the mixing section of chlorination reactor；S3, dispersing agent is added in the conversion zone of chlorination reactor, 50~120 DEG C is then heated to, under ultraviolet light, the melting ethylene carbonate in S2 is added, then the chlorine being then passed through in S1 reacts 4h at 50~120 DEG C, after reaction, chlorizate is obtained.The present invention provides a kind of chloridization process of ethylene carbonate, it is reacted by using dispersing agent with ultraviolet coupling, avoid using it is ultraviolet it is light-initiated be unevenly distributed because of chlorine caused by side reaction increase, the problem of yield fluctuation of chlorocarbonic acid vinyl acetate, improve the content of chlorocarbonic acid vinyl acetate.
Description
Technical field
The present invention relates to chlorocarbonic acid vinyl acetate synthesis technical fields, and in particular to a kind of chlorination work of ethylene carbonate
Skill.
Background technique
Chlorocarbonic acid vinyl acetate (chloroethylene carbonate；Chloroethyleneglycol
Carbonate), Chinese nickname: chloro- 1, the 3- dioxolane -2- ketone (4-chloro-1,3-dioxolan-2-one) of 4-.Chloro
Ethylene carbonate, which is mainly used in, prepares lithium battery electrolytes fluorinated ethylene carbonate and vinylene carbonate.High-purity chloro is for carbon
Vinyl acetate can also improve the cycle performance of lithium battery electrolytes directly as lithium battery electrolytes flame-retardant additive, improve
Service life.
The existing chlorocarbonic acid vinyl acetate technology for preparing exists because by-products content is more caused by chlorine dispersion is uneven, reaction effect
Rate is low, and product purity is low；In addition, byproduct of reaction cannot be effectively addressed, environmental pollution will cause.Therefore, it is necessary to open
It is less toxic to send out a kind of, purification is efficient, method is simple, is suitble to a kind of chloridization process of ethylene carbonate of industrialized production.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of chloridization process of ethylene carbonate, special
Sign is, comprising the following steps:
S1, liquid chlorine vaporizing is obtained into chlorine, be then fed into chlorination reactor mixing section；
S2, ethylene carbonate is preheated at 36~40 DEG C, obtains melting ethylene carbonate, and be added to chlorination reactor
In mixing section；
S3, the conversion zone that dispersing agent is added to chlorination reactor, are then heated to 50~120 DEG C, under ultraviolet light,
The melting ethylene carbonate in S2 in chlorination reactor mixing section is added, is then passed through the chlorine in S1 in chlorination reactor mixing section
Then gas reacts 4h at 50~120 DEG C, after reaction, obtain chlorizate；Wherein, chlorine and melting ethylene carbonate
Mass ratio be 1.0~1.5:1.
Preferably, in step S2, the water content of the ethylene carbonate is less than 10ppm.
Preferably, in step S3, the dispersing agent is polyalkylene glycol alkyl amine, and the quality of dispersing agent is melting carbonic acid second
The 5~20% of enester quality.
Preferably, in step S3, the flow of the chlorine is 1~10ml/h.
Preferably, in step S3, the chlorine is passed through process point three Duan Jinhang, specifically, when temperature of reactor is 50~
At 80 DEG C, it is passed through the 25% of chlorine total amount, when temperature of reactor is 80~90 DEG C, the 45% of chlorine total amount is passed through, works as reaction
When device temperature is 90~150 DEG C, it is passed through the 30% of chlorine total amount.
Preferably, in step S3, the exposure intensity of the ultraviolet light is 30000uw/cm2。
Compared with prior art, the present invention the beneficial effect is that:
(1) ethylene carbonate ester chloridization process provided by the invention is reacted with ultraviolet coupling using dispersing agent, avoids purple
It is outer it is light-initiated be unevenly distributed because of chlorine caused by side reaction increase, the problem of the yield fluctuation of chlorocarbonic acid vinyl acetate, improve
The content of chlorocarbonic acid vinyl acetate.
(2) the chlorocarbonic acid ethylene ester content in synthetic product of the present invention reaches as high as 87%, the conversion of ethylene carbonate
Rate reaches as high as 97.2%.
(3) reaction condition of the present invention is mild, and reaction process Environmental Safety, no especial equipment requirements.
Specific embodiment
In order to enable those skilled in the art to more fully understand, technical solution of the present invention is practiced, below with reference to specific
The invention will be further described for embodiment, but illustrated embodiment is not as a limitation of the invention.
The test method of actual conditions is not specified in following embodiments, according to conventional methods in the art with condition into
Row, raw materials used is commercially available.
In following embodiment step S2, the water content of the ethylene carbonate used is less than 10ppm.
Embodiment 1
A kind of chloridization process of ethylene carbonate, specifically includes the following steps:
S1, liquid chlorine is entered into Chlorine Buffer Vessel after the gasification of chlorine evaporator, and be sent in the mixing section of chlorination reactor；
Wherein, chlorine evaporator is heated using 0.4MPa low-pressure steam；
S2, ethylene carbonate is preheated at 36 DEG C, melting ethylene carbonate is obtained, then by the melting carbonic acid second of 100g
Enester is added in the mixing section of chlorination reactor；
S3,5g polyalkylene glycol alkyl amine is added in the conversion zone of chlorination reactor by solid feed inlet；Then will
Reactor is heated to 50 DEG C, starts ultraviolet lamp, and under ultraviolet light, the melting carbon in S2 in chlorination reactor mixing section is added
Vinyl acetate is then passed through the chlorine in S1 in chlorination reactor mixing section, then reacts 4h at 50~100 DEG C；
Wherein, the process that is passed through of chlorine is carried out in three steps: the first step, when reaction temperature is 50 DEG C, is passed through chlorine total amount
25%, the flow of chlorine is 5ml/h, reacts 1h；It is total to be passed through chlorine when reaction temperature is then adjusted to 80 DEG C for second step
The 45% of amount, the flow of chlorine are 9ml/h, the reaction was continued 1h；Third step is passed through when reaction temperature continues to be adjusted to 100 DEG C
The 30% of chlorine total amount, the flow of chlorine are 4ml/h, the reaction was continued 2h；Chlorizate 142.8g is obtained after reaction.Its
In, in step S3, the mass ratio of chlorine and melting ethylene carbonate is 1.32:1.
By carrying out GC detection to chlorizate obtained above, testing result is shown, chlorocarbonic acid second in chlorizate
Enester content 84%, ethylene carbonate content 5.5%, dichloro- ethylene carbonate content 5.1%, the conversion ratio of ethylene carbonate
94.5%.
Embodiment 2
A kind of chloridization process of ethylene carbonate, specifically includes the following steps:
S1, liquid chlorine is entered into Chlorine Buffer Vessel after the gasification of chlorine evaporator, and be sent in the mixing section of chlorination reactor；
Wherein, chlorine evaporator is heated using 0.4MPa low-pressure steam；
S2, ethylene carbonate is preheated at 38 DEG C, melting ethylene carbonate is obtained, then by the melting carbonic acid second of 100g
Enester is added in the mixing section of chlorination reactor；
S3,10g polyalkylene glycol alkyl amine is added in the conversion zone of chlorination reactor by solid feed inlet；Then will
Reactor is heated to 80 DEG C, starts ultraviolet lamp, and under ultraviolet light, the melting carbon in S2 in chlorination reactor mixing section is added
Vinyl acetate is then passed through the chlorine in S1 in chlorination reactor mixing section, then reacts 4h at 80~110 DEG C；
Wherein, the process that is passed through of chlorine is carried out in three steps: the first step, when reaction temperature is 80 DEG C, is passed through chlorine total amount
25%, the flow of chlorine is 7ml/h, reacts 1h；It is total to be passed through chlorine when reaction temperature is then adjusted to 90 DEG C for second step
The 45% of amount, the flow of chlorine are 8ml/h, the reaction was continued 1h；Third step is passed through when reaction temperature continues to be adjusted to 110 DEG C
The 30% of chlorine total amount, the flow of chlorine are 3ml/h, the reaction was continued 2h；Chlorizate 146.3g is obtained after reaction.Its
In, in step S3, the mass ratio of chlorine and melting ethylene carbonate is 1.26:1.
By carrying out GC detection to chlorizate obtained above, testing result is shown, chlorocarbonic acid second in chlorizate
Enester content 84.8%, ethylene carbonate content 4.8%, dichloro- ethylene carbonate content 5.8%, the conversion of ethylene carbonate
Rate 95.2%.
Embodiment 3
A kind of chloridization process of ethylene carbonate, specifically includes the following steps:
S1, liquid chlorine is entered into Chlorine Buffer Vessel after the gasification of chlorine evaporator, and be sent in the mixing section of chlorination reactor；
Wherein, chlorine evaporator is heated using 0.4MPa low-pressure steam；
S2, ethylene carbonate is preheated at 40 DEG C, melting ethylene carbonate is obtained, then by the melting carbonic acid second of 100g
Enester is added in the mixing section of chlorination reactor；
S3,7.5g polyalkylene glycol alkyl amine is added in the conversion zone of chlorination reactor by solid feed inlet；Then
Reactor is heated to 70 DEG C, starts ultraviolet lamp, under ultraviolet light, the melting in S2 in chlorination reactor mixing section is added
Ethylene carbonate is then passed through the chlorine in S1 in chlorination reactor mixing section, then reacts 4h at 70~100 DEG C；
Wherein, the process that is passed through of chlorine is carried out in three steps: the first step, when reaction temperature is 70 DEG C, is passed through chlorine total amount
25%, the flow of chlorine is 7ml/h, reacts 1h；It is total to be passed through chlorine when reaction temperature is then adjusted to 90 DEG C for second step
The 45% of amount, the flow of chlorine are 8ml/h, the reaction was continued 1h；Third step is passed through when reaction temperature continues to be adjusted to 100 DEG C
The 30% of chlorine total amount, the flow of chlorine are 5ml/h, the reaction was continued 2h；Chlorizate 144.5g is obtained after reaction.Its
In, in step S3, the mass ratio of chlorine and melting ethylene carbonate is 1.5:1.
By carrying out GC detection to chlorizate obtained above, testing result is shown, chlorocarbonic acid second in chlorizate
Enester content 84.8%, ethylene carbonate content 4.2%, dichloro- ethylene carbonate content 5.3%, the conversion of ethylene carbonate
Rate 95.8%.
Embodiment 4
A kind of chloridization process of ethylene carbonate, specifically includes the following steps:
S1, liquid chlorine is entered into Chlorine Buffer Vessel after the gasification of chlorine evaporator, it is spare, and it is sent to the mixing of chlorination reactor
Duan Zhong；
Wherein, chlorine evaporator is heated using 0.4MPa low-pressure steam；
S2, ethylene carbonate is preheated at 36 DEG C, melting ethylene carbonate is obtained, then by the melting carbonic acid second of 100g
Enester is added in the mixing section of chlorination reactor；
S3,7.5g polyalkylene glycol alkyl amine is added in the conversion zone of chlorination reactor by solid feed inlet；Then
Reactor is heated to 90 DEG C, starts ultraviolet lamp, under ultraviolet light, the melting in S2 in chlorination reactor mixing section is added
Ethylene carbonate is then passed through the chlorine in S1 in chlorination reactor mixing section, then reacts 4h at 90~95 DEG C；
Wherein, the process that is passed through of chlorine is carried out in three steps: the first step, when reaction temperature is 90 DEG C, is passed through chlorine total amount
25%, the flow of chlorine is 7ml/h, reacts 1h；Reaction temperature is continued to remain 90 DEG C, is passed through chlorine total amount by second step
45%, the flow of chlorine is 8ml/h, the reaction was continued 1h；Third step is passed through chlorine when reaction temperature continues to be adjusted to 95 DEG C
The 30% of gas total amount, the flow of chlorine are 5ml/h, the reaction was continued 2h；Chlorizate 146.5g is obtained after reaction.Wherein,
In step S3, the mass ratio of chlorine and melting ethylene carbonate is 1.5:1.
By carrying out GC detection to chlorizate obtained above, testing result is shown, chlorocarbonic acid second in chlorizate
Enester content 85.3%, ethylene carbonate content 3.5%, dichloro- ethylene carbonate content 5.8%, the conversion of ethylene carbonate
Rate 96.5%.
Embodiment 5
A kind of chloridization process of ethylene carbonate, specifically includes the following steps:
S1, liquid chlorine is entered into Chlorine Buffer Vessel after the gasification of chlorine evaporator, and be sent in the mixing section of chlorination reactor；
Wherein, chlorine evaporator is heated using 0.4MPa low-pressure steam；
S2, ethylene carbonate is preheated at 40 DEG C, melting ethylene carbonate is obtained, then by the melting carbonic acid second of 100g
Enester is added in the mixing section of chlorination reactor；
S3,20g polyalkylene glycol alkyl amine is added in the conversion zone of chlorination reactor by solid feed inlet；Then will
Reactor is heated to 80 DEG C, starts ultraviolet lamp, and under ultraviolet light, the melting carbon in S2 in chlorination reactor mixing section is added
Vinyl acetate is then passed through the chlorine in S1 in chlorination reactor mixing section, then reacts 4h at 80~105 DEG C；
Wherein, the process that is passed through of chlorine is carried out in three steps: the first step, when reaction temperature is 80 DEG C, is passed through chlorine total amount
25%, the flow of chlorine is 6ml/h, reacts 1h；It is total to be passed through chlorine when reaction temperature is then adjusted to 90 DEG C for second step
The 45% of amount, the flow of chlorine are 8ml/h, the reaction was continued 1h；Third step is passed through when reaction temperature continues to be adjusted to 105 DEG C
The 30% of chlorine total amount, the flow of chlorine are 3ml/h, the reaction was continued 2h；Chlorizate 145.5g is obtained after reaction.Its
In, in step S3, the mass ratio of chlorine and melting ethylene carbonate is 1.2:1.
By carrying out GC detection to chlorizate obtained above, testing result is shown, chlorocarbonic acid second in chlorizate
Enester content 87.2%, ethylene carbonate content 4.9%, dichloro- ethylene carbonate content 5.6%, the conversion of ethylene carbonate
Rate 95.1%.
Embodiment 6
A kind of chloridization process of ethylene carbonate, specifically includes the following steps:
S1, liquid chlorine is entered into Chlorine Buffer Vessel after the gasification of chlorine evaporator, and be sent in the mixing section of chlorination reactor；
Wherein, chlorine evaporator is heated using 0.4MPa low-pressure steam；
S2, ethylene carbonate is preheated at 36 DEG C, melting ethylene carbonate is obtained, then by the melting carbonic acid second of 100g
Enester is added in the mixing section of chlorination reactor；
S3,5g polyalkylene glycol alkyl amine is added in the conversion zone of chlorination reactor by solid feed inlet；Then will
Reactor is heated to 85 DEG C, starts ultraviolet lamp, and under ultraviolet light, the melting carbon in S2 in chlorination reactor mixing section is added
Vinyl acetate is then passed through the chlorine in S1 in chlorination reactor mixing section, then reacts 4h at 85~120 DEG C；
Wherein, the process that is passed through of chlorine is carried out in three steps: the first step, when reaction temperature is 85 DEG C, is passed through chlorine total amount
25%, the flow of chlorine is 8ml/h, reacts 1h；It is total to be passed through chlorine when reaction temperature is then adjusted to 95 DEG C for second step
The 45% of amount, the flow of chlorine are 8ml/h, the reaction was continued 1h；Third step is passed through when reaction temperature continues to be adjusted to 120 DEG C
The 30% of chlorine total amount, the flow of chlorine are 3ml/h, the reaction was continued 2h；Chlorizate 143.3g is obtained after reaction.Its
In, in step S3, the mass ratio of chlorine and melting ethylene carbonate is 1.32:1.
By carrying out GC detection to chlorizate obtained above, testing result is shown, chlorocarbonic acid second in chlorizate
Enester content 85.8%, ethylene carbonate content 2.8%, dichloro- ethylene carbonate content 6.2%, the conversion of ethylene carbonate
Rate 97.2%.
In conclusion when the chlorocarbonic acid ethylene ester content in synthetic product of the embodiment of the present invention reaches as high as 87%, carbon
The conversion ratio of vinyl acetate reaches as high as 97.2%, and product purity is high.
It should be noted that involved in claims of the present invention when numberical range, it is thus understood that each numberical range
Any one numerical value can be selected between two endpoints and two endpoints, due to step method and the embodiment 1-6 phase of use
Together, it repeats in order to prevent, the present invention describes preferred embodiment, and once a person skilled in the art knows basic wounds
The property made concept, then additional changes and modifications may be made to these embodiments.So the following claims are intended to be interpreted as includes
Preferred embodiment and all change and modification for falling into the scope of the invention.
Obviously, various changes and modifications can be made to the invention without departing from essence of the invention by those skilled in the art
Mind and range.In this way, if these modifications and changes of the present invention belongs to the range of the claims in the present invention and its equivalent technologies
Within, then the present invention is also intended to include these modifications and variations.
Claims (6)
1. a kind of chloridization process of ethylene carbonate, which comprises the following steps:
S1, liquid chlorine vaporizing is obtained into chlorine, be then fed into chlorination reactor mixing section；
S2, ethylene carbonate is preheated at 36~40 DEG C, obtains melting ethylene carbonate, and be added to the mixed of chlorination reactor
It closes in section；
S3, dispersing agent is added in the conversion zone of chlorination reactor, is then heated to 50~120 DEG C, under ultraviolet light, adds
Enter the melting ethylene carbonate in S2 in chlorination reactor mixing section, is then passed through the chlorine in S1 in chlorination reactor mixing section
Then gas reacts 4h at 50~120 DEG C, after reaction, obtain chlorizate；Wherein, chlorine and melting ethylene carbonate
Mass ratio be 1.0~1.5:1.
2. the chloridization process of ethylene carbonate according to claim 1, which is characterized in that in step S2, the carbonic acid second
The water content of enester is less than 10ppm.
3. the chloridization process of ethylene carbonate according to claim 1, which is characterized in that in step S3, the dispersing agent
For polyalkylene glycol alkyl amine, and the quality of dispersing agent is melt ethylene carbonate quality 5~20%.
4. the chloridization process of ethylene carbonate according to claim 1, which is characterized in that in step S3, the chlorine
Flow is 1~10ml/h.
5. the chloridization process of ethylene carbonate according to claim 1, which is characterized in that in step S3, the chlorine is logical
Enter three Duan Jinhang of process point, specifically, being passed through the 25% of chlorine total amount when temperature of reactor is 50~80 DEG C, working as reactor
When temperature is 80~90 DEG C, it is passed through the 45% of chlorine total amount, when temperature of reactor is 90~120 DEG C, is passed through chlorine total amount
30%.
6. the chloridization process of ethylene carbonate according to claim 1, which is characterized in that in step S3, the ultraviolet light
Exposure intensity be 30000uw/cm2。
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Cited By (3)
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| CN112979607A (en) * | 2021-03-11 | 2021-06-18 | 泰兴华盛精细化工有限公司 | Method for continuously preparing chlorinated ethylene carbonate |
| CN113402494A (en) * | 2021-06-19 | 2021-09-17 | 济宁正旺生物科技有限公司 | Method for improving yield of chlorinated ethylene carbonate |
| CN115286612A (en) * | 2022-07-27 | 2022-11-04 | 珠海正杏新材料科技有限公司 | Production method of chloroethylene carbonate |
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| CN112979607A (en) * | 2021-03-11 | 2021-06-18 | 泰兴华盛精细化工有限公司 | Method for continuously preparing chlorinated ethylene carbonate |
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Application publication date: 20191112 |